Moberg My, Bergquist Jonas, Bylund Dan
Analytical Chemistry, Department of Physical and Analytical Chemistry, Uppsala University, SE-751 24 Uppsala, Sweden.
J Mass Spectrom. 2006 Oct;41(10):1334-45. doi: 10.1002/jms.1108.
The feasibility and advantages of using sophisticated chemometric tools in combination with the execution of thoroughly planned experiments to determine experimental conditions for optimal performance of an LC-ESI-MS/MS analysis is demonstrated. A stepwise strategy is proposed, which provides a controlled optimization procedure of the chromatographic quality (in terms of separation among the sample constituents) and maximizes the mass spectrometric signal of the selected product ions. Design of experiments (DOE) and response surface methodology are applied throughout the procedure. The stepwise approach has the advantage of dealing with the different optimization criteria separately, i.e. first ensuring sufficient chromatographic separation, then maximizing the amount of precursor ion entering the mass spectrometer, and finally generating high amounts of selected product ions. The experiments are performed on a linear ion trap mass spectrometer. Retention mapping using the band-tracking model is applied during LC development, which facilitates the optimization of segmented gradients. A set of different siderophores, strong iron chelates, is used as the model substances.
本文展示了结合使用精密化学计量工具和精心设计的实验来确定液相色谱-电喷雾串联质谱（LC-ESI-MS/MS）分析最佳性能实验条件的可行性和优势。提出了一种逐步策略，该策略提供了色谱质量（就样品成分之间的分离而言）的可控优化程序，并使所选产物离子的质谱信号最大化。在整个过程中应用了实验设计（DOE）和响应面方法。逐步方法的优点是分别处理不同的优化标准，即首先确保足够的色谱分离，然后使进入质谱仪的前体离子量最大化，最后产生大量的所选产物离子。实验在线性离子阱质谱仪上进行。在液相色谱方法开发过程中应用了基于谱带追踪模型的保留时间映射，这有助于分段梯度的优化。一组不同的铁载体，即强铁螯合物，用作模型物质。
